Department of Forensic Science COPYRIGHT © 2021 CONTROLLEDVIRGINIA SUBSTANCES PROCEDURESDEPARTMENT MANUAL OF FORENSIC SCIENCE 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 1 of 176 COPY Table of Contents TABLE OF CONTENTS 1 Introduction 1.1 Introduction 1.2 Examination Documentation 2 Analytical Schemes 2.1 Introduction 2.2 Determination of Quantity 2.3 General Unknowns/Powders/Illicit Tablets 2.4 Tablets and Capsules 2.5 Cannabis 2.6 Pharmaceutical Identifiers 2.7 Color Tests 2.8 Chromatography 2.9 Infrared Spectroscopy/MassCOPYRIGHT Spectrometry © 2021 2.10 Further Testing 2.11 Liquids 2.12 Plant Material 3 Drug Item Reduction Program VIRGINIA 3.1 Introduction DEPARTMENT 3.2 Procedures 4 Weighing Practices OF 4.1 Procedures FORENSIC SCIENCE 4.2 Weighing Practices 4.3 References 5 Sampling 5.1 Introduction 5.2 General Sampling 5.3 Administrative Sampling Plan 5.4 Hypergeometric Sampling Plan 5.5 Multiple Specimens 5.6 Bulk Materials 5.7 Residue Samples 5.8 Sampling for Quantitative Analysis 5.9 References 6 Cannabis Plant Material 6.1 Introduction 6.2 Macroscopic Identification 6.3 Microscopic Identification 6.4 4-Aminophenol (4-AP) Color Test 6.5 Duquenois-Levine 6.6 Thin Layer Chromatography (TLC) 6.7 DART-TOF 6.8 Semi-quantitative Gas Chromatography-Flame Ionization-Mass Spectrometry (GC-FID-MS) 6.9 Quantitative Analysis of Total THC in Plant Material using GC/MS (SIM) 6.10 Residues 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 2 of 176 COPY Table of Contents 6.11 References 7 Cannabis Extracts and Products 7.1 Introduction 7.2 Cannabis Extracts 7.3 Extraction of THC from Food Products (candy, brownies, etc.) 7.4 Cannabinoid Quantitation by High Performance Liquid Chromatography – Diode Array Detection (HPLC-DAD) 7.5 References 8 Pharmaceutical Identifiers (PI) 8.1 Introduction 8.2 Procedure 9 Color Tests COPYRIGHT © 2021 9.1 Introduction 9.2 Procedures 9.3 Color Tests and Reagents 9.4 References VIRGINIA 10 Thin Layer Chromatography DEPARTMENT 10.1 Introduction 10.2 Materials 10.3 Methods OF 10.4 TLC Baths 10.5 Visualization ReagentsFORENSIC SCIENCE 10.6 Preparative Thin Layer Chromatography 10.7 Comparative Semi-Quantitative Thin Layer Chromatography 10.8 References 11 Gas Chromatography 11.1 Introduction 11.2 Materials 11.3 Methods 11.4 Quantitation 12 High Performance Liquid Chromatography (HPLC) 12.1 Introduction 12.2 Materials 12.3 Methods 12.4 Quantitation 13 Analysis of Pharmaceutical Injectable Dosage Forms 13.1 Introduction 13.2 Procedure 13.3 Reporting 14 Infrared Spectroscopy 14.1 Introduction 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 3 of 176 COPY Table of Contents 14.2 Sample Preparation 14.3 Solid State FTIR via Gas Chromatography 14.4 Acceptance Criteria 15 Gas Chromatography/Mass Spectrometry 15.1 Introduction 15.2 Procedure 15.3 Data Interpretation and Acceptance Criteria 16 DART-TOF Mass Spectrometry 16.1 Introduction 16.2 General Drug Screening Method 16.3 Negative Screening Method including GHB 16.4 Pharmaceutical Confirmation via DART-TOF 16.5 References COPYRIGHT © 2021 17 General Analytical Methodology 17.1 Introduction 17.2 Techniques VIRGINIA 17.3 Reference Collections 17.4 Structural Similarity EvaluationDEPARTMENT 17.5 Guidelines for Quantitative Method Validation and Verification 18 Stimulant Methodology OF 18.1 Brief PharmacologyFORENSIC SCIENCE 18.2 Drug Group Examples 18.3 Types of Samples 18.4 Scheduling 18.5 Extraction 18.6 Color Test Results 18.7 TLC 18.8 GC 18.9 GC/MS 18.10 FTIR 18.11 Amphetamine/Methamphetamine Quantitation 18.12 Differentiation of the Stereoisomers of Methamphetamine using GC Derivatization (Determination of “ICE”) 19 Cocaine and Local Anesthetic Methodology 19.1 Brief Pharmacology 19.2 Drug Group Examples 19.3 Scheduling 19.4 Extraction 19.5 Color Test Results 19.6 TLC 19.7 FTIR 19.8 Cocaine Quantitation 20 Barbiturate Methodology 20.1 Brief Pharmacology 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 4 of 176 COPY Table of Contents 20.2 Drug Group Examples 20.3 Types of Samples 20.4 Scheduling 20.5 Extraction 20.6 Color Test Results 20.7 TLC 20.8 GC 20.9 GC/MS 20.10 FTIR 21 Narcotic Methodology 21.1 Brief Pharmacology 21.2 Drug Group Examples 21.3 Scheduling 21.4 Extraction 21.5 Color Test Results 21.6 TLC COPYRIGHT © 2021 21.7 Dextromethorphan Enantiomer Determination 21.8 Heroin Quantitation 22 Phencyclidine (PCP) and Analog MethodologyVIRGINIA 22.1 Brief Pharmacology 22.2 Scheduling DEPARTMENT 22.3 Extraction 22.4 Color Test Results 22.5 TLC OF 22.6 GC 22.7 FTIR FORENSIC SCIENCE 22.8 PCP Quantitation 23 Lysergic Acid Diethylamide (LSD) Methodology 23.1 Scheduling 23.2 Analog 23.3 Extraction 23.4 Color Test Results 23.5 TLC 23.6 GC 23.7 FTIR 24 Mescaline Methodology 24.1 Scheduling 24.2 Extraction 24.3 Color Test Results 24.4 TLC 25 Psilocybin and Psilocyn Methodology 25.1 Scheduling 25.2 Extractions 25.3 Color Test Results 25.4 TLC 25.5 GC 25.6 FTIR 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 5 of 176 COPY Table of Contents 26 Cathinone Methodology 26.1 Scheduling 26.2 Sample Handling 26.3 Extraction 26.4 TLC 26.5 GC/MS 26.6 References 27 MDA/MDMA Methodology 27.1 Scheduling 27.2 Color Test Results 27.3 TLC 27.4 GC 27.5 FTIR 27.6 MDMA QuantitationCOPYRIGHT © 2021 28 Anabolic Steroid Methodology 28.1 Brief Pharmacology 28.2 Drug Group Examples VIRGINIA 28.3 Scheduling 28.4 Extraction DEPARTMENT 28.5 Color Test Results 28.6 Pharmaceutical Identifiers 28.7 TLC OF 28.8 GC 28.9 FTIR FORENSIC SCIENCE 28.10 GC/MS 28.11 References 29 GHB Methodology 29.1 Brief Pharmacology 29.2 Drug Group Examples 29.3 Scheduling 29.4 Chemical Properties 29.5 pH 29.6 Color Test Results 29.7 TLC 29.8 GC 29.9 GC/MS 29.10 FTIR 29.11 References 30 Salvinorin A Methodology 30.1 Scheduling 30.2 Extractions 30.3 TLC 30.4 GC and GC/MS 30.5 Reporting 30.6 References 31 Cannabimimetic Agent Methodology 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 6 of 176 COPY Table of Contents 31.1 Scheduling 31.2 Extractions 31.3 TLC 31.4 GC and GC/MS 31.5 References 32 Clandestine Laboratories 32.1 Introduction 32.2 Analytical Approach 32.3 Procedure 32.4 References 33 Estimation of the Uncertainty of Measurement (UoM) 33.1 Scope 33.2 Uncertainty ElementsCOPYRIGHT © 2021 33.3 Weights 33.4 Determination of Uncertainty of Measurement for Extrapolation Cases 33.5 Case File Records and Reporting for Weights 33.6 Measurement Traceability 33.7 Quantitations VIRGINIA 33.8 References DEPARTMENT 34 Reporting Guidelines 35 Drug Reversals OF 35.1 Introduction FORENSIC SCIENCE 35.2 Procedure 36 Quality Assurance 36.1 Introduction 36.2 Reagents 36.3 Standards 36.4 Balances 36.5 Thin Layer Chromatography 36.6 Gas Chromatographs 36.7 Liquid Chromatographs 36.8 Mass Spectrometers 36.9 FTIR 36.10 DART-TOF 36.11 Refrigerators/Freezers 36.12 DiscovIR GC-FTIR 36.13 Glassware 36.14 Mechanical Pipettes 37 Bibliography 38 Scheduling 38.1 Schedule I 38.2 Schedule II 38.3 Schedule III 38.4 Schedule IV 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 7 of 176 COPY Table of Contents 38.5 Schedule V 38.6 Schedule VI 39 Weight Thresholds 40 Hypergeometric Table 41 Commonly Used Abbreviations COPYRIGHT © 2021 VIRGINIA DEPARTMENT OF FORENSIC SCIENCE 221-D100 Controlled Substances Procedures Manual Qualtrax ID: 2480 Issued by Chemistry Program Manager UNCONTROLLED Qualtrax Revision 18 Issue Date: 18-August-2021 Page 8 of 176 COPY 1 Introduction 1 INTRODUCTION 1.1 Introduction The information in this Procedures Manual was collected from numerous sources and is presented here for easy reference for drug chemists. In all cases, it is acceptable to use the most current edition of listed literature references. This manual presents a basic outline of the types of drugs analyzed, a source book on reagent and standard preparation and a description of the analytical techniques used with a review of instrumentation. This manual is not all-inclusive, and will reference other sources where appropriate. It is always the chemist's responsibility to choose the best analytical scheme for each individual case. It is expected that supervisors will be consulted for extraordinary procedures. 1.2 Examination Documentation 1.2.1 Specific worksheets are provided as controlled forms and should be used as designed. Examination documentation must contain sufficient detail to allow another examiner to repeat the analysis under conditions as close as possible to the original, evaluate the data, interpret the results and come to the same conclusion. COPYRIGHT © 2021 1.2.2 The General Drug Worksheet is a generic worksheet for controlled substances casework. The comments section should be used for explanations of tests or lists of weights, etc. 1.2.3 The Blank Worksheet is availableVIRGINIA for cases requiring more notes than will easily fit on the General Drug Worksheet.